Method of making coke



Reissued Dec. 3, 1940 UNITED STATES I -Re. 21,651

METHOD OF MAKING COKE Earl W. Rice, St; Paul,

Iowa,

Buchele, Iowa City,

Minn, and Walter J. assignors of sixty-six and two-thirds per cent to Courtney W. Kimler, Sr., and Harry Ball, Ames, Iowa No Drawing. Original No.

ber 24, 1939, Serial No. Application for reissue rialNo. 355,218 g 5 Claims.

The object of our invention is to aiford a method of making coke which consists broadly in adding to petroleum carbon coke fines or breeze a proper amount of pitch derived from the by- 5 products coke industry, having the characteristics hereinafter mentioned and charging the mixture into a vertical by-product coke oven and subjecting same to coking temperature until practicaliy all volatile gases have been driven oil! and i coking action is completed.

ing of the ingredients and treatment of the mixture as hereinafter more fully set forth.

' Petroleum coke is a product of the oil distillation or cracking process as now practiced in the petroleum industry. A great-percentage of petroleum coke is produced or recovered in the fine state or in what is called breeze form. These lines are difficult to market in their present state.

20 They are smoky, greasy and dirty to handle.

The fines are produced by the method of extraction from the stills; where chains, balls and other means are used to break up the accumulation of coke in the stills, as fast as possible to save time in clearing the stills and to make them quickly ready for the next run. What is wanted is.gasoline, not coke. It readily resolves itself down to the point that the petroleum coke is a necessary so evil of the oil cracking process and must be removed as quickly as possible regardless oi the state or form of the resultant product. There is available a great quantity of this coke breeze for which there is no market.

The pitch used is a resultant of coal tar and by-product coking processes, and is used in a refined state. The melting point of the pitch must be such that the mixture will not eiiervesce excessively and form out the vents of the coke oven 0 and thus clog up the vents when charged into ovens carrying a coking temperature.-

The temperature at which the pitch will effervesce will vary. In that we mean a pitch of lower melting temperature can be used if the ovens are kept at 1800" F., than if oven temperature of 2200" is used. Lower melting point pitch can be used in a 14" oven and oven temperature 'of l800 than would be necessary to use in a 14" oven with 2200 temperature. This means that a wide variation in melting range of pitch can be used and one must use the pitch best adapted to the temperature and width of oven. And the final qualification of the pitch used is that it wlllnot eflervesce and clog the.

as vents of the oven when charged into coking oven Our invention consists in the selection and mix- 2,111,226, dated Octozoaszs, May 2:. 1938. September 3, 1940, Se-

at coking temperature or during the coking process.

A great many unsuccessful attempts have been made to utilize petroleum coke breeze and form it into hard solid pieces of a size adapted to metallurgical and domestic use. In fact we were discouraged by many coke producers 'who stated that they had spent hundreds of thousands of dollars trying to do what we claimed we could do.

At the plant where our tests were run, the results of which will appear later, we had to guarantee them against damage to ovens. Then they were so pessimistic and suspicious of our process, and our inability to push the finished product from the ovens that we had to start with /4 charge of our materials and A charge of byproduct materials. Finally we used /2, then /4 of our materials and less by-product in proportion, then a full charge of our material, and amperage on pusher was not raised.

We use a mixture of from 50% to 95% petroleum coke breeze to form 50% to 5% pitch in a fine state thoroughly mixed, and charge same into a vertical by-product coke oven and seal same against admission of air which is ordinary coking practice; subject the charge to a coking temperature until coking action is completed. Then vents are opened and charge pushed into the quenching car where it is quenched, which is also ordinary coking practice.

In our test a core pitch with a melting point of 284 F. was used. Core pitch can be secured with a melting range between 270 and 315 F. But

not eflervesce excessively and be used. Petroleum pitches any pitch that will clog the oven can commonly called asphalts have the same chemical composition as coal tar pitches and therefore may be used. They are available in proper quantities.

If a coke having some volatile gases is desired, the coking action can be stopped and charge pushed out before all gases are distilled ofi.

' If a hard, dense metallurgical coke is desired, the action can be carried to completion and practically all volatile gases eliminated with a resultapproximately as follows: 99.19% fixed C.; 37% ash; .44% volatile (and .65% sulphur).

' The lengthof coking time depends on oven temperature, width of oven, capacity of oven,

etc.

In our tests a temperature of between 1700 and 1854 F. was used in a 1'1" oven on a coking time of approximately 32 hours, with excellent results.

If the oven is narrowed this coking time can be reduced, and if temperature is raised, the

coking time will be reduced. If both the temperature is raised and the oven narrowed, the coking. time can be materially decreased until it is possible to secure a coking cycle of between 4 to 8 hours.

We use a vertical by-product coke oven be-' oven the dust loss or lines are practically negligible.

our process is a practical process and produces a high grade, hard coke, ot cially' adapted to high grade metallurgical use. It can also be used domestically as our tests have proven.

This product is a high grade metallurgical coke, high in fixed carbon. low in volatile and ash. with a sulphur content adapted to metallurgical processes. The coke is a new product differing distinctly from petroleum coke or pitch. the original ingredients, in that it is higher in fixed carbon, lower in volatile and ash. and much harder and more firm in structure.

It has specific gravity of approximately 1.85.

It can-be pushed through the oven without difflculty and comes out hard, solid, and of good size.

. ,By this method we have Its hardness ranges from 80 to 300 by A. St T. ll. hardness test and will carry a very heavy burden. which makes it particularly valuable in the steel and metallurgical industry.

taken two low priced. nearly waste products and produced a finished coke having a-commercial value of about twice that of its ingredientswith a 105 of about 13%. Never heretofore has a high grade metallurgical cofleolbeen produced by ticailerely putting' beether pe cum coke and pi only and subjecting, them to a coking temperature in a ertlcal byproduct coke oven for the proper This may be became dinary pitches,

goodsise and es'pereaction time depends upon the size of the retort used, the quantity of material and similar discretionary factors.

Samples of the coke made in accordance with the present invention have been subjected to laboratory tests ior chemical composition and physical characteristics. Samples taken from one representative batch of this new synthetic fuel showed the following analysis:

Thephysical characteristics oithis product were tested by the Standard Tumbler Test method. This consists in placing the coke in a drum 5 feet in diameter and 30 inches long and making 50 revolutions of the drum. The case of the drum is perforated with 2%-inch openings. One hundred pounds of material is charged into the drum. The results were as follows:

Tania: No. 3 r I Tumbler test of experimental cordancemwith thepresent in'vaihtion. ihae ex- B c E, perimen runsweremade core ltehm 100x X R m. r wh-W'i'A'l' -l49.5

TaarnNal PM .m '71: me: any cum m rail im M. M 'r. a 1.2:: t: a a: c 1 2am an ion 8.1 -U 1 s a :2: e: :...M"' :1! In 17 l a "as 1).. um are nsu as a I. name ..l8-IDo. I abouldbenotedtbattbepru entinventlm (r-0+mx1oo-4' .bepracticeduflliaing telling (m n 'Td 1m to m P. III! 1m m b. 1w p 3 mtforaperiodottimeranaingi'rma'amt ii 4 acreen)=1'.85

The chemical analyses of the product of other runs wasas follows:

Tasha No. 5

A. S. T. M. comparative method, pieces were 7 squared by cutting them with a hack-saw. They were faced with plaster of Paris before being placed in a compression testing machine. They were then tested in the same manner as concrete cubes. The following table is representative of the results obtained:

Tum No. 6

' Absolute structural strenyth Cube sire Ultimate strength 7 Lbs. per Dimensions To l m-sinhas? i, 102 1, 4a) 957 997 l, 134

These ultimate strength values are quite com- 5 parable to the ultimate strength values desired for high grade metallurgical fuelsmade from coal. It has never been possible to manufacture a coke from these materials that carries the necessary sizing and has this structural strength 50 value. In fact a fuel produced in accordance with the present invention has a structural strength which is more than double the structural strength of any previously prepared fuel of this general character.

This, application is a continuation-in-part of applicants application Serial No. 132,594, filed March 24, 1937.

It is to be understood that, although some par-' ticular compositions embodying the present invention and methods of producing'the same and also some of the arts inwhich the present invention may be utilized have been set forth and discussed vention is above. nevertheless the present innot limited to the exact ingredients or artamentioned. the scope of 'saidinvention being commensurate with the following claims.

proportionsortotheprecisemethodsofthoseproduct coke oven and subjecting same to a cokproduct coke oven and subjecting same to a cokjing temperature until coking action is completed. producing a metallurgical coke having approxiing a melting point such that it will not eifervesce l. A method of producing a metallurgical coke from petroleum coke consisting of the mixing of petroleum coke breeze or fines, with pitch derived from the by-product coke or coal tar industry in the proportion of from 50% to 95% by weight 5 of petroleum coke breeze or fines and 50% to 5% by weight of pitch in fine state and charging same into a vertical by-product coke oven and subjecting to a coking temperature until coking action is completed, producing a metallurgical coke having approximately the following analysis:

99.19% F. C.; 37% ash, .44% volatile and .65% sulphur.

2. A method of producing a metallurgical coke from petroleum coke consisting of the mixing of petroleum coke breeze or fines with core pitch" in the proportion of 50% to 95% petroleum coke breeze or fines with from 50% to 5% "core pitc in fine state, charging same into a vertical bying temperature until coking action is completed, producing a metallurgical coke having approximately the following analysis: 99.19% F. C.; 37% ash, .44% volatile and .65% sulphur.

3. A method of producing a metallurgical coke from petroleum coke consisting of mixing of petroleum coke breeze or fines with pitch derived from the distillation of coal tars and having a melting point such that it will not effervesce excessively and clog the oven vents, in the proportion of 50% to 95% petroleum coke breeze or fines with from 50% to 5% of said pitch in a fine state, charging said mixture into a vertical bymately the following analysis: 99.19% F. '0 .37% ash, .44% volatile and .65,% sulphur.

4. A method ofproducing a metallurgical coke from petroleum coke consisting of the mixing of petroleum coke breeze or fines, with pitch derived from the lay-product coke or coal tar industry. in the proportion of from'50% to 95% by weight of petroleum coke breeze or fines and 50% to 5% by weight of pitch in fine state and charging same into a lay-product coke oven and subjecting to a coking temperature until coking action is completed, producing a metallurgical coke having approximately the following analysis: 99.19% F. 0.; 37% ash, 44% volatile and 55% sulphur.

5. A method of producing a metallurgical coke from petroleum coke consisting of the mixing of petroleum coke breeze or fines with pitch havexcessively and clog the oven vents,,in the proportion of to'95 petroleum coke breeze or fines with from 50% to 5% of said pitchin a fine state, charging saidmlxture into a coking oven and subjecting same to a coking temperature until coking action is completed, producing a metallurgical coke having approximatelythe following analysis: Not less than 97% F. C.; not more than 2% volatilematterpnot less than.

mm. W. arcs. ,WAL'I'ER. J. BUCHELE. 

